CN109679324A - Low temperature resistant wear-resisting TPU composite material and preparation method for nailed climbing boots - Google Patents
Low temperature resistant wear-resisting TPU composite material and preparation method for nailed climbing boots Download PDFInfo
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- CN109679324A CN109679324A CN201811601179.0A CN201811601179A CN109679324A CN 109679324 A CN109679324 A CN 109679324A CN 201811601179 A CN201811601179 A CN 201811601179A CN 109679324 A CN109679324 A CN 109679324A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/017—Additives being an antistatic agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Footwear And Its Accessory, Manufacturing Method And Apparatuses (AREA)
Abstract
The present invention relates to a kind of low temperature resistant wear-resisting TPU composite material and preparation methods for nailed climbing boots, belong to polyurethanes technology field.TPU composite material of the present invention, the raw material including following weight percentage: TPU master batch 80-92%, ABS resin 5-13%, modified Nano carbon fiber 0.1~0.5%, hydrolysis agent 0.1~0.5%, antioxidant 0.1~0.5%, polyvinyl fluoride 1~5%, polyethylene wax 0.2~0.5%；The TPU master batch is with oligomeric polyols, diisocyanate, chain extender and Nano-meter SiO_22For raw material, prepared by double screw extruder.TPU composite material of the present invention not only has excellent wear-resisting and resistance to low temperature, but also has good mechanical property and resilience, and stability is splendid in process of production, can be widely applied for footwear material field；Invention also provides simple and easy preparation methods.
Description
Technical field
The present invention relates to a kind of low temperature resistant wear-resisting TPU composite material and preparation methods for nailed climbing boots, belong to poly- ammonia
Ester technical field.
Background technique
Thermoplastic polyurethane elastomer (TPU) is a kind of high molecular polymer of function admirable, has had both the elasticity of rubber
With the hardness of plastics, but also have good machining property, wearability and resilience performance, be widely used in tubing,
The fields such as auto parts and components, footwear material.
At present in climbing boot field, TPU has been widely used in shoes outsole and shoes accessory, but since TPU is hypocrystalline
Block polymer make its friction containing a large amount of highly polar group such as carbamate groups, ester group and urea groups in molecular structure
Coefficient is high, and electric conductivity is poor, and intensity, thermal stability and glass transition temperature are difficult to adapt to extreme mountain environment and wind and snow
Weather, therefore the application of footwear material sole is restricted outdoors.
The method for usually improving TPU resistance to low temperature mainly uses the polyalcohol of resistance to low temperature to improve, but its intensity
The method for being extremely difficult to require, and improving TPU wear-resisting property with toughness is to utilize auxiliary agent or inorganic material with anti-attrition function
Blending and modifying is carried out to TPU, but inorganic material and the compatibility of polyurethane are poor, is easy to cause material that phase point occurs after blending
From mechanical strength declines to a great extent.Therefore, while improving TPU composite-material abrasive, resistance to low temperature, guarantee it with good
Good intensity and machining property, peomotes TPU composite material in the application in the field for having high abrasion requirement.
Summary of the invention
The object of the present invention is to provide a kind of low temperature resistant wear-resisting TPU composite materials for nailed climbing boots, not only have excellent
Different wear-resisting and resistance to low temperature, and there is good mechanical property and resilience, stability is splendid in process of production,
It can be widely applied for footwear material field；Invention also provides simple and easy preparation methods.
Low temperature resistant wear-resisting TPU composite material of the present invention for nailed climbing boots, including following weight percentage
Raw material:
The TPU master batch is with oligomeric polyols, diisocyanate, chain extender and Nano-meter SiO_22For raw material, pass through double spiral shells
Bar squeezes out machine one-step method preparation, and the shore hardness of TPU master batch is 60A~60D, and particle size is 3~6mm.
When using twin-screw extrusion, plasticizer is added in the 9th area of screw rod back segment.Plasticizer is the aliphatic two of low smell
One or both of first esters of gallic acid, Phthalates or benzoates.
The oligomeric polyols are polyoxyethylated polyols, polyoxypropylene polyol, polycaprolactone polyol or poly-
One or both of tetramethylene adipate polyalcohol, number-average molecular weight 1000-2000.
The diisocyanate is 4,4'- methyl diphenylene diisocyanate, toluene di-isocyanate(TDI), 1,4- cyclohexyl-
Diisocyanate or hexamethylene diisocyanate.
The small molecular alcohol chain extender is one of 1,4- butanediol, ethylene glycol, 1,3- propylene glycol or 1,6-HD
Or two kinds.
The Nano-meter SiO_22Partial size is 50-200nm.
Preferably, TPU master batch is made of the raw material of following weight percentage:
The modified Nano carbon fiber is to be prepared by chemical vapour deposition technique, then passes through silane coupler modified system
?.It is specific the preparation method is as follows:
Carbon nano-fiber, silane coupling agent, dehydrated alcohol and deionized water are mixed into ultrasonic disperse, then heating carries out silicon
Alkylation reaction, whole process are passed through N2, finally washed with dehydrated alcohol, suction filtration handles to obtain the modified Nano carbon fiber.
The hydrolysis agent is the one or two of single second carbide imine or polycarbodiimide.
The antioxidant is Hinered phenols antioxidant or phosphite ester antioxidant.
The preparation method of the low temperature resistant wear-resisting TPU composite material for nailed climbing boots, comprising the following steps:
(1) using oligomeric polyols, diisocyanate and chain extender as raw material, material temperature is controlled at 95-120 DEG C, is vacuumized and is removed
Moisture sequentially adds light stabilizer, release agent, Nano-meter SiO_2 in oligomeric polyols2, material kettle opens stirring, beats circulation；Pass through
Metering pump realizes that oligomeric polyols and chain extender carry out quantitative premix, while catalyst dilutes (temperature of charge through polyether polyol
It is 45-60 DEG C), by metering pump metered the firstth area of double screw extruder sprue gate, plasticizer passes through spiral shell by metering pump
The 9th area's exhaust outlet of bar is added, 12 warm area settings 160/190/190/190/180/170/160/140/140/140/ of screw rod
150/160 DEG C, material reacts 70-90s through bulk polymerization, and reaction product is cut granulating system under water, 0.1%- is added in water tank
The silicone oil antistatic agent of 0.5% mass fraction, the elastomer particles ultimately produced under the conditions of 85-105 DEG C, are dried in vacuo 6-
10h obtains the TPU master batch；
(2) TPU master batch, ABS resin, modified Nano carbon fiber, hydrolysis agent, antioxidant, polyvinyl fluoride and poly- second are weighed
Alkene wax, is first placed in high speed mixing smelting machine and mixes, and adds and carries out extruding pelletization in double screw extruder, institute is obtained after vacuum drying
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots stated.
The catalyst and the mass ratio of polyether polyol are 0.0125-0.02:1.
The catalyst is stannous octoate or bismuth neodecanoate；Polyether polyol is polyoxypropylene polyol, data molecule
Amount is 1000.
The light stabilizer is one of benzophenone class, benzotriazole or hindered amines or a variety of.
The release agent is stearic acid or polyamide-based lubricant.
Compared with prior art, the invention has the following advantages:
(1) present invention has the TPU master batch of resistance to low temperature by synthesis, so that final TPU composite material tool obtained
There is excellent resistance to low temperature；
(2) present invention is effectively improved between TPU molecule segment by introducing ABS resin, polyvinyl fluoride and polyethylene wax
Lubricity significantly improves its wear-resisting property；
(3) in the TPU master batch that the present invention synthesizes, the highly polar group of carbamate groups and polyvinyl fluoride forms hydrogen bond,
So that the degree of disorder of TPU strand increases, to significantly reduce the glass transition temperature of TPU, and then the resistance to of TPU composite material is improved
Cryogenic property；
(4) invention introduces Nano-meter SiO_2s2, modified carbon nano tube fiber, effectively increase the mechanical property of TPU, improve
The problem of antistatic property deficiency；
(5) present invention is during synthesizing TPU master batch, using one-step method production process, chain extender and oligomeric polyols
It is added after premix, it can be with the mixed effect of strength imparting material；Catalyst is added after polyether polyol dilutes through specific metering pump,
The regulation that online reactivity may be implemented, is adjusted for different product, reduces the generation of side reaction；Plasticizer is in double spiral shells
The 9th area of bar back segment is added, and can effectively reduce the reaction that moisture and free hydroxyl group in plasticizer participate in NCO, effectively promotion product
Stability；
(6) TPU composite material prepared by the present invention, reachable -70 DEG C of brittle temperature, abrasion loss is 25~35mm3, resist
Electrostatic factors are down to 107；
(7) preparation method of TPU composite material of the present invention, it is simple and easy, it is conducive to industrialized production.
Specific embodiment
Below with reference to embodiment, the present invention is further illustrated, but it is not intended to limit implementation of the invention.
The percentage being previously mentioned below is mass percentage.
Embodiment 1
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 36%, r value (NCO/OH molar ratio) 1.005；
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, preparation process are as follows:
1) using oligomeric polyols, diisocyanate and small molecule glycol as raw material, material temperature is controlled at 95-120 DEG C, is vacuumized
Moisture removal sequentially adds light stabilizer, release agent, Nano-meter SiO_2 in oligomeric polyols2, material kettle opens stirring, beats circulation；It is oligomeric
After polyalcohol and chain extender premix, each component is injected into double screw extruder together, while environment-friendly type catalyst is through polyoxygenated
Propylene polyalcohol dilution (thinner ratio 1:80, temperature of charge are 45-60 DEG C), is squeezed by the metered twin-screw of dedicated metering pump
The firstth area of machine sprue gate out, low smell plasticizer P B805 are added by metering pump in the 9th area of screw rod back segment, and material is through ontology
Polymerization, reacts 70-90s, and reaction product is cut granulating system under water, the silicone oil of 0.1%-1% mass fraction is added in water tank
Antistatic agent, the elastomer particles ultimately produced under the conditions of 85-105 DEG C, are dried in vacuo 6-10h；
2) TPU master batch, ABS resin, modified Nano carbon fiber, hydrolysis agent, antioxidant, polyvinyl fluoride, polyethylene are weighed
Wax is placed in high speed mixing smelting machine and is sufficiently mixed, and adds double screw extruder and carries out extruding pelletization；It is produced after vacuum drying
Product.
Embodiment 2
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 36%, r value (NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical.
Embodiment 3
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 36%, r value (NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical.
Embodiment 4
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 46%, r value (NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical.
Embodiment 5
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, and number-average molecular weight is 2000, react hard section 59%, r value
(NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical.
Comparative example 1
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 36%, r value (NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical.
Comparative example 2
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 36%, r value (NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical.
Comparative example 3
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 36%, r value (NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical, remove plasticizer additional equipment, and plasticizer is added in oligomeric polyols kettle and mixes
It closes and participates in reaction；
Comparative example 4
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, poly adipate succinic acid ester (mass ratio 1:1), the equal molecule of number
Amount is 2000, reacts hard section 46%, r value (NCO/OH molar ratio) 1.005；
Preparation process and embodiment 1 are identical；
Comparative example 5
The low temperature resistant wear-resisting TPU composite material for nailed climbing boots, the raw material including following weight percentage:
Wherein TPU master batch is made of the raw material of following weight percentage:
The oligomeric polyols are polycaprolactone polyol, and number-average molecular weight is 2000, react hard section 59%, r value
(NCO/OH molar ratio) 1.005；
Such as table 1 of polyurethane elastomer product performance obtained by each embodiment and comparative example.
Tensile strength is tested by high-speed rail tensilon；
Glass transition temperature is tested by the dsc analysis instrument of PE company；
Abrasion are with the test of DIN equipment standard；
5% thermal weight loss is in N2Under atmosphere, tested by TG analyzer.
The performance indicator of 1 TPU composite material of table is as follows
The Nano-meter SiO_2 that the present invention introduces simultaneously it can be seen from 1 data of table2, ABS resin, modified carbon nano tube fiber, have
Effect promotes TPU mechanical property, antistatic property, overcomes the disadvantage of heat resistance deficiency, and polyvinyl fluoride, polyethylene wax, can be with
The lubricity between TPU molecule segment is effectively improved, its wear-resisting property is significantly improved, isocyanate group and polyvinyl fluoride in TPU
Highly polar group form hydrogen bond so that the degree of disorder of TPU strand increases, to significantly reduce the glass transition temperature of TPU, into
And improve the resistance to low temperature of TPU composite material.Furthermore low the 9th area of smell plasticizer back segment is individually added into and can effectively reduce
Moisture and free hydroxyl group participate in the reaction of NCO in plasticizer, effectively promote properties of product and production stability.
Claims (10)
1. a kind of low temperature resistant wear-resisting TPU composite material for nailed climbing boots, it is characterised in that: including following weight percentage
Raw material:
The TPU master batch is with oligomeric polyols, diisocyanate, chain extender and Nano-meter SiO_22For raw material, pass through twin-screw extrusion
Machine preparation.
2. the low temperature resistant wear-resisting TPU composite material according to claim 1 for nailed climbing boots, it is characterised in that: using double
When Screw Extrusion, plasticizer is added in the 9th area of screw rod back segment.
3. the low temperature resistant wear-resisting TPU composite material according to claim 1 for nailed climbing boots, it is characterised in that: oligomeric more
First alcohol is that polyoxyethylated polyols, polyoxypropylene polyol, polycaprolactone polyol or poly adipate succinic acid ester are polynary
One or both of alcohol, number-average molecular weight 1000-2000.
4. the low temperature resistant wear-resisting TPU composite material according to claim 1 for nailed climbing boots, it is characterised in that: modification is received
Rice carbon fiber is prepared by chemical vapour deposition technique, is made by silane coupler modified.
5. the low temperature resistant wear-resisting TPU composite material according to claim 1 for nailed climbing boots, it is characterised in that: hydrolysis
Agent is the one or two of single second carbide imine or polycarbodiimide.
6. the low temperature resistant wear-resisting TPU composite material according to claim 1 for nailed climbing boots, it is characterised in that: antioxidant
For Hinered phenols antioxidant or phosphite ester antioxidant.
7. a kind of preparation method of any low temperature resistant wear-resisting TPU composite material for nailed climbing boots of claim 1-6,
Be characterized in that the following steps are included:
(1) using oligomeric polyols, diisocyanate and chain extender as raw material, sequentially added in oligomeric polyols light stabilizer,
Release agent, Nano-meter SiO_22, realize that oligomeric polyols and chain extender carry out quantitative premix by metering pump, while catalyst is through polyethers
Polyalcohol dilution, by the metered double screw extruder of metering pump, plasticizer is vented by metering pump by the 9th area of screw rod
Mouth is added, and reacts 70-90s, is cut granulation under water, obtains the TPU master batch；
(2) TPU master batch, ABS resin, modified Nano carbon fiber, hydrolysis agent, antioxidant, polyvinyl fluoride and polyethylene wax are weighed,
It is first placed in high speed mixing smelting machine and mixes, add and carry out extruding pelletization in double screw extruder, obtained after vacuum drying described
Low temperature resistant wear-resisting TPU composite material for nailed climbing boots.
8. the preparation method of the low temperature resistant wear-resisting TPU composite material according to claim 7 for nailed climbing boots, feature exist
In: catalyst and the mass ratio of polyether polyol be 0.0125-0.02:1.
9. the preparation method of the low temperature resistant wear-resisting TPU composite material according to claim 8 for nailed climbing boots, feature exist
In: catalyst is stannous octoate or bismuth neodecanoate；Polyether polyol is polyoxypropylene polyol, number average molecular weight 1000.
10. the preparation method of the low temperature resistant wear-resisting TPU composite material according to claim 7 for nailed climbing boots, feature
Be: light stabilizer is one of benzophenone class, benzotriazole or hindered amines or a variety of；Release agent is stearic acid or gathers
Amide series lubricant agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269552A (en) * | 2020-03-18 | 2020-06-12 | 广州钰鑫新材料有限公司 | Anti-skid wear-resistant shoe material and preparation method thereof |
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